ANION SELF-REGENERATING SUPPRESSOR 300 (ASRS 300 (4-mm), P/N ) (ASRS 300 (2-mm), P/N )

Transcription

1 ASRS 300 CSRS 300

2 SRS 300 Product Manual Page 1 of 50 PRODUCT MANUAL FOR THE ANION SELF-REGENERATING SUPPRESSOR 300 (ASRS 300 (4-mm), P/N ) (ASRS 300 (2-mm), P/N ) CATION SELF-REGENERATING SUPPRESSOR 300 (CSRS 300 (4-mm), P/N ) (CSRS 300 (2-mm), P/N ) Dionex Corporation, 2008 Document No Revision 06 August 2008

3 SRS 300 Product Manual Page 2 of 50 TABLE OF CONTENTS 1. INTRODUCTION Self-Regenerating Suppressor Overview of Suppression Modes Mode of Operation Selection The AutoSuppression Recycle Mode The AutoSuppression External Water Mode The Chemical Suppression Mode The MPIC Suppression Mode INSTALLATION System Requirements Self-Regenerating Suppressor Control Reagent-Free Controller (RFC) Back Pressure Coils for the SRS Assembly Gas Separator Waste Tube for the SRS Assembly Self-Regenerating Suppressor Current Selection Calculating the Optimum Current Setting OPERATION Chemical Purity Requirements Inorganic Chemicals Solvents Deionized Water Start-up Hydration Back Pressure Coil Pressure Test Quick Back Pressure Check Plumbing for the AutoSuppression Recycle Mode Operation Eluent Flow Path Connections in the AutoSuppression Recycle Mode Regenerant Flow Path Connections in the AutoSuppression Recycle Mode Installation in Thermal Chamber Installation in ICS Plumbing for the AutoSuppression External Water Mode Operation Eluent Flow Path Connections for the AutoSuppression External Water Mode Regenerant Flow Path Connections in the AutoSuppression External Water Mode Regenerant Flow Path Connections in the AutoSuppression External Water Mode with Peristaltic Pump Installation in Thermal Chamber Installation in ICS Plumbing for Chemical Suppression Mode Operation Plumbing for MPIC Suppression Mode Operation Eluent Flow Path Connections in MPIC Suppression Mode Regenerant Flow Path Connections in MPIC Suppression Mode Using Pressurized Water Delivery System MPIC Suppression Mode Operation Self-Regenerating Suppressor (SRS 300) Storage Short Term Storage (1 to 5 days) Long Term Storage (More than 5 days) TROUBLESHOOTING GUIDE Self-Regenerating Suppressor Operational Status Displays Alarm State Small or Increasing Analyte Peak Areas Suppressor Regeneration Steps Full or Extended Regeneration: High Background Conductivity Drifting Baseline Noisy Baseline Decreased Sensitivity System Back Pressure Increases Over Time Liquid Leaks Poor or unstable recovery of certain peaks Peaks and spikes in the absence of an injection... 34

4 SRS 300 Product Manual Page 3 of SELF-REGENERATING SUPPRESSOR CLEANUP Metal Contaminants or Precipitates Organic Contaminants APPENDIX A - CURRENT SETTINGS...37 A.1. Optimum Current Settings for Common Eluents; ASRS 300 (4 and 2 mm) A.2 Optimum Current Settings for Common Eluents; CSRS 300 (4 and 2 mm) A.3 Current Settings for Older Detectors APPENDIX B - SUPPRESSOR CONTROLLER...42 B.1 SRS Control for the CD20/CD25/CD25A and ED40/ED50/ED50A (DX-500 instruments) B.1.1 SRS Control for the DX B.1.2 SRS Control for the CDM-3/PED-2 (DX-300 Instruments) B.1.3 SRS Control for the DX-100 (Model DX 1-03) B.1.4 SRC Controller APPENDIX C - ALARM STATES FOR OLDER INSTRUMENTS...47 C.1 Alarm States for the CD20/ED40 (DX-500 Instruments) C.1.1 Alarm States for the DX C.1.2 Alarm States for The CDM-3 and PED-2 (DX-300 Instruments), DX-100 (Model 1-03) and SRC ATTACHMENT - SRS 300 QUICKSTART...49

5 SRS 300 Product Manual Page 4 of INTRODUCTION 1.1. Self-Regenerating Suppressor The Self-Regenerating Suppressor (SRS 300) replaces the ULTRA II suppressor product line. The SRS 300 is redesigned with exterior hardware changes that allow the suppressor to be more pressure tolerant than previous generation suppressor devices. The SRS 300 continues to use cleaned ion exchange components (gasketed screens and membranes) as the ULTRA II suppressor devices. The 2mm ASRS 300 replaces the ASRS MS suppressor product and should be used for anion Mass Spectrometry (MS) Applications. The Self-Regenerating Suppressor 300 (SRS 300) is available in two versions: the Anion Self-Regenerating Suppressor 300 (ASRS 300) or Cation Self-Regenerating Suppressor 300 (CSRS 300). The SRS 300 system consists of a Self-Regenerating Suppressor, the SRS Control, the back pressure coils, and the Gas Separator Waste Tube. This high performance, low maintenance AutoSuppression system provides a reliable solution for Ion Chromatography. Additionally, the SRS 300 offers high capacity suppression while adding minimal dead volume to the analytical system. The ASRS 300 provides continuous suppression of traditional eluents, and more concentrated eluents up to 200 mm NaOH. The CSRS 300 offers continuous suppression of concentrated eluents up to 100 mn H 2 SO 4 or MSA. This high capacity significantly expands the capabilities and simplifies the operation of Ion Chromatography. The SRS 300 is available in both 2-mm and 4-mm formats for use with 2, 3, 4, or 5-mm Ion Chromatography columns and systems. The 2-mm SRS 300 is specially designed with reduced internal volume to ensure optimum performance with 2-mm columns and systems. In fact, the suppression capacity of the 2-mm version is greater than the 4-mm version due to the reduced eluent flow rate and proportionally greater surface area. Anion Self-Regenerating ) Suppressor (ASRS 300 Waste Gas Separator Waste Tube 1/ Coil # Coi #1 l Back Pressure Coils or 1/4-28 Figure 1 The Self-Regenerating Suppressor Assistance is available for any problem during the shipment or operation of Dionex products through the Dionex North America Technical Call Center at DIONEX-0 ( ) or through any of the Worldwide Dionex Offices on the Reference Library CD-ROM.

6 SRS 300 Product Manual Page 5 of 50 The SRS 300 design comprises of two regenerant chambers and one eluent chamber separated by ion exchange membranes. Regenerant flow chambers and an eluent flow chamber are defined by the gasketed screens. The eluent flows countercurrent to the regenerant. Electrodes are placed along the length of the regenerant chambers. When an electric potential is applied across the electrodes, water from the regenerant chambers is electrolyzed, supplying regenerant hydronium ions (H 3 O + ) in the ASRS 300 and regenerant hydroxide ions (OH - ) in the CSRS 300 for the neutralization reaction. The membrane allows hydronium or hydroxide ions to pass into the eluent chamber resulting in the conversion of the electrolyte of the eluent to a weakly ionized form. Eluent counter ions (cations in anion exchange or anions in cation exchange) are simultaneously passed into the regenerant chamber to maintain charge balance. The eluent suppression process is illustrated for Anion Suppressor in Figure 2 and for Cation Suppressor in Figure 3. As shown in Figure 2, the water regenerant undergoes electrolysis to form hydrogen gas and hydroxide ions in the cathode chamber while oxygen gas and hydronium ions are formed in the anode chamber. In the Anion Suppressor, cation exchange membranes allow hydronium ions to move from the anode chamber into the eluent chamber to neutralize hydroxide. Sodium ions in the eluent, attracted by the electric potential applied, move across the membrane into the cathode chamber to maintain electro neutrality and combine with the hydroxide ions generated at the cathode. Thus effecting suppression of the eluent and conversion of the analyte to typically a more conductive acid form. ASRS 300 in AutoSuppression Mode ANODE + Waste/Vent ANALYTE IN Na + OH - ELUENT (NaOH) CATHODE Waste/Vent - H 2 O + O 2 Na + OH - + H 2 H 3 O + Na + OH - OH - 2H 3 O + + ½ O 2 (g) H H OH - 2 O 3H 2 O 2 H 2 O ANALYTE IN H 2 O H 2 O H 2 O TO DETECTOR Figure 2 AutoSuppression with the ASRS 300

7 SRS 300 Product Manual Page 6 of 50 As shown in Figure 3, the water regenerant undergoes electrolysis to form hydrogen gas and hydroxide ions in the cathode chamber while oxygen gas and hydronium ions are formed in the anode chamber. In the cation suppressor, anion exchange membranes allow hydroxide ions to move from the cathode chamber into the eluent chamber to neutralize hydronium ions. Anions in the eluent, such as methane sulfonate, attracted by the electric potential applied, move across the membrane into the anode chamber to maintain electro neutrality and combine with the hydronium ions generated at the anode. Thus effecting suppression of the eluent and conversion of the analyte to typically a more conductive base form. CSRS 300 in AutoSuppression Mode ANODE + Waste/Vent ANALYTE IN H + MSA - ELUENT (MSA) CATHODE Waste/Vent - MSA + O 2 H 2 O + H 2 H + + MSA - MSA - + H + OH - [H + + OH - ] 2H 3 O + + ½ O 2 (g) H H OH - 2 O 3H 2 O 2 H 2 O ANALYTE IN H 2 O H 2 O H 2 O TO DETECTOR Figure 3 AutoSuppression with the CSRS 300 The ASRS 2 mm suppressor is compatible with the MS and replaces the ASRS MS suppressor product. The suppressor has been designed to have minimal sulfate interference for MS applications. The 2 mm suppressor is recommended for MS applications due to the improved efficiency, and since less eluent enters the MS at the relatively lower operational flow rate.

8 SRS 300 Product Manual Page 7 of Overview of Suppression Modes Four basic modes of suppression can be performed with the Self-Regenerating Suppressor (SRS 300): AutoSuppression Recycle Mode AutoSuppression External Water Mode Chemical Suppression Mode MPIC Suppression Mode AutoSuppression Recycle Mode: The SRS 300 uses water as the regenerant for eluent suppression. There are two modes of electrolytic operation. The most simple and recommended mode of operation is the AutoSuppression Recycle Mode. In this mode of operation, eluent flows from the eluent outlet of the suppressor into the conductivity cell and is then recycled through the SRS 300 regenerant chambers. This eliminates the need for an external source of regenerant water but limits the regenerant flow rate to the eluent flow rate. The AutoSuppression Recycle Mode is the most common mode of operation and is recommended for aqueous eluents. AutoSuppression External Water Mode: This mode incorporates an external source of deionized water flowing through the regenerant chambers. The detector cell effluent is directed to waste. This requires the installation of pressurized bottle system or additional pump to provide an external source of water. With this configuration the regenerant flow rate is not limited to the eluent flow rate. The AutoSuppression External Water mode is primarily recommended with solvent containing eluents (up to 40%) Chemical Suppression Mode: The Chemical Suppression Mode is a non-electrolytic mode of operation and therefore requires no power supply. This mode of operation requires the installation of equipment (either the AutoRegen Accessory equipped with a AutoRegen Regenerant Cartridge, a pressurized bottle delivery system or additional pump, or a Displacement Chemical Regeneration (DCR) Kit). This system delivers sulfuric acid to the ASRS 300 suppressor or tetrabutylammonium hydroxide (TBAOH) to the CSRS 300 suppressor regenerant chambers. MPIC Suppression Mode: The MPIC Suppression Mode is a combination of the AutoSuppression External Water Mode augmented with a chemical regenerant such as sulfuric acid (ASRS 300) or boric acid (CSRS 300). When the SRS 300 is operating in this mode, it uses an applied current and a constant source of dilute regenerant solution from a pressurized bottle delivery system or additional pump. The following sections explain how each mode works and help to determine which mode to use for an application. Once the mode of operation is determined, more detailed plumbing configuration and operating instructions can be found in Section 3, Operation Mode of Operation Selection The SRS 300 mode of operation depends mainly on your eluent composition and your analysis sensitivity requirements. The compatibilities are shown in Table 1. For example, eluents containing organic solvents are not compatible with the AutoSuppression Recycle Mode. The AutoSuppression External Water Mode or Chemical Suppression Mode should be used instead. The MPIC Suppression Mode is specifically designed for applications where ion-pair reagents and solvents are present in the eluent. Table 1 Eluent Composition and Suppression Mode Compatibility Eluent Composition Suppression Recycle Suppression External Water Chemical Suppression MPIC Suppression Aqueous Eluents Yes Yes Yes N/A Eluents Containing No Yes (Up to 40%) Yes (Up to 100%) N/A Organic Solvents Eluents Containing Ion Pair Reagents with/without Solvents No No No Yes

9 SRS 300 Product Manual Page 8 of The AutoSuppression Recycle Mode The AutoSuppression Recycle Mode uses the neutralized conductivity cell effluent as the source of water for the regenerant chamber water. This is the preferred method of operation for the SRS 300. The advantage of this mode of operation is simplicity and ease of use. This mode reliably provides AutoSuppression for most suppressed conductivity applications using solvent-free eluents. As the eluent passes through the SRS 300, it is neutralized to its weakly ionized form. After passing through the conductivity cell, the effluent is redirected to the regenerant inlet on the SRS 300, thus supplying it with a source of water containing minute amounts of diluted analyte. The amount of water flowing through the regenerant chambers is therefore limited to the eluent flow rate. See Section 3 for complete operating instructions The AutoSuppression External Water Mode The AutoSuppression External Water Mode is used for any application requiring organic solvents in the eluent or sample. This mode uses a constant source of deionized water from a pressurized bottle or other source of deionized water that delivers 1 to 2 ml/min for 2-mm applications and 3-5 ml/min for 4-mm applications. The amount of water flowing through the regenerant chambers is therefore independent of the eluent flow rate. The AutoSuppression External Water Mode eliminates the potential for build-up of contaminating ions resulting from the oxidation of solvents. It also reliably provides AutoSuppression for high sensitivity analysis, maximizing signal-to-noise ratios for suppressed conductivity applications. Any analysis performed using the AutoSuppression Recycle Mode can also be performed using the AutoSuppression External Water Mode. See Section 3 for complete operating instructions The Chemical Suppression Mode Dionex recommends the use of a MicroMembrane Suppressor (MMS 300) for chemical suppression applications. The SRS 300 can also be used in the Chemical Suppression Mode. The chemical suppression mode should be used for applications using 40% (V/V), or greater solvent or where the lowest noise is required. In this mode no power or current is applied. The Anion Chemical Suppression Mode uses sulfuric acid (H 2 SO 4 ) as a chemical regenerant and the Cation Chemical Suppression Mode uses tetrabutylammonium hydroxide (TBAOH) as a chemical regenerant. Dionex recommends for typical anion applications a sulfuric acid regenerant concentration between 25 mn and 75 mn and for typical cation applications a TBAOH regenerant concentration of between 50 mn and 100 mn. It should be noted that there will be a small leakage of regenerant ions into the eluent channel and is dependent primarily on the concentration of the regenerant used. A lower regenerant concentration is preferred at a relatively higher flow rate since it produces a lower level of leakage hence a lower background, than a higher regenerant concentration at a lower flow rate. In the Chemical Suppression Mode, the SRS 300 is operated exactly like a MicroMembrane Suppressor (MMS 300). Regenerant is supplied to the regenerant chambers from a Dionex AutoRegen Accessory or a pressurized bottle delivery system or additional pump or a Displacement Chemical Regeneration (DCR) Kit. See Section 3 for complete operating instructions or refer to the MMS Manual Document No and the DCR Kit Manual Document No

10 SRS 300 Product Manual Page 9 of 50 Chemical Suppression with the ASRS 300 is a neutralization reaction and selective desalting process carried out across the cation exchange membranes. In this mode, no electric potential is applied across the electrodes. Hydronium ions in the chemical regenerant cross the membranes and combine with the basic eluent anions (in this case hydroxide) to form water. At the same time, eluent cations cross the membranes into the regenerant stream replacing the hydronium ions. ASRS 300 in Chemical Suppression Mode ANALYTE IN Na + OH - Waste/Vent ELUENT Waste/Vent Na + + HSO 4 - Na + + HSO 4 - Na + Na + H + H + + OH - H + H 2 O HSO 4 - HSO 4 - ANALYTE IN H 2 O H - + HSO 4 - H - + HSO 4 - TO DETECTOR Figure 4 Chemical Suppression with the ASRS 300 NOTE Do not plug the ASRS 300 to the SRS power supply

11 SRS 300 Product Manual Page 10 of 50 Chemical Suppression with the CSRS 300 is a neutralization reaction and selective desalting process carried out across the anion exchange membranes. In this mode no electric potential is applied across the electrodes. Hydroxide ions in the chemical regenerant cross the membranes and combine with the acidic eluent cations, in this case hydronium ion, to form water. At the same time, eluent anions cross the membranes into the regenerant stream replacing the hydroxide ions. CSRS 300 in Chemical Suppression Mode ANALYTE IN H + MSA - Waste/Vent ELUENT Waste/Vent TBA + + MSA - TBA + + MSA - MSA - MSA - OH - H + + OH - OH - H 2 O TBA + TBA + ANALYTE IN H 2 O TBA + + OH - TBA + + OH - TO DETECTOR Figure 5 Chemical Suppression with the CSRS 300 NOTE Do not plug the CSRS 300 to the SRS power supply

12 SRS 300 Product Manual Page 11 of The MPIC Suppression Mode Anion MPIC The ASRS 300 is used for eluent suppression of Mobile Phase Ion Chromatography (MPIC or ion-pairing) eluents by using the MPIC Suppression Mode. The MPIC Suppression Mode is a combination of the AutoSuppression External Water Mode augmented with a chemical regenerant such as sulfuric acid (H 2 SO 4 ). The MPIC Suppression Mode uses an applied current and a constant source of dilute sulfuric acid solution from a pressurized bottle delivery system. This mode must be used for MPIC applications requiring an ion pair reagent and organic solvents in the eluent. The MPIC Suppression Mode reliably provides suppression of typical eluents for MPIC applications using suppressed conductivity detection. The ion pair reagents, such as tetrabutylammonium hydroxide (TBAOH), are used in concentrations typically ranging from 1.0 to 5.0 mm. See Section 3 for complete operating instructions Cation MPIC The CSRS 300 is used for eluent suppression of MPIC eluents by using the AutoSuppression External Water Mode or the MPIC Suppression Mode depending on the specific MPIC application. The MPIC Suppression Mode uses an applied current and a constant source of dilute boric acid regenerant solution from a pressurized bottle delivery system. Dilute boric acid is added to the water regenerant to enhance detection and improve linearity of weak bases such as ammonia and amines. This mode is used for MPIC applications requiring an ion pair reagent and organic solvents in the eluent. The MPIC Suppression Mode reliably provides suppression of typical eluents for MPIC applications using suppressed conductivity detection. The ion pair reagents, such as octanesulfonic acid (OSA), are used in concentrations typically ranging from 1.0 to 5.0 mm. Organic solvent concentrations should not exceed 40%. See Section 3 for complete operating instructions.

13 SRS 300 Product Manual Page 12 of INSTALLATION 2.1. System Requirements The SRS 300 is designed to be run on any Dionex Ion Chromatography System (ICS) equipped with a Anion or Cation exchange column set and suppressed conductivity detection. The ICS-2500, ICS-2000, and ICS-1500 systems are fully capable of controlling the suppressor from either the front panel touch screen or from Chromeleon software. The ICS-1000 and ICS-3000 systems control the suppressor only through Chromeleon software. DX-500 systems with a CD20 or ED40 Detector; DX-120 systems; DX-300 systems having a Conductivity Detector Module (CDM-3) or a Pulsed Electrochemical Detector (PED-2); and the DX-100 (Model DX 1-03) contain SRS Control integrated into the detector. Older systems require a standalone controller such as the SCR-1, SC20, RFC-10, or RFC-30 Controller for installation of the SRS 300. See Table 2, Self-Regenerating Suppressor Requirements for Selected ICS Modules. The older SRC-1 controller has been discontinued. The replacement product is either the RFC-10 controller or the RFC-30 controller. The RFC-10 controller provides 1 ma graduated control of an electrolytic suppressor. The RFC-30 controller also provides 1 ma graduated control and, in addition, provides control of an Eluent Generator Cartridge (EGC) and a Continuously Regenerated Trap Column (CR-TC). It is highly recommended to set the current setting for the SRS 300 to the exact calculated current (within 1 ma). Older power supplies do not have the 1 ma graduated control. For older systems it is recommended to upgrade to a newer power supply such as the RFC-10 or RFC-30. Failure to set the current accurately could reduce performance. Table 2 Self-Regenerating Suppressor Requirements for Selected Ion Chromatographs Ion Chromatograph Series Module RFC-10 or RFC-30 Controller Requirement 2000i YES QIC YES 2000 SP YES 4000i YES 4500i YES 8000 YES 8100 N/A 8200 N/A DX-100 YES Model DX 1-03 RECOMMENDED DX-120 RECOMMENDED DX-300 N/A CDM-2, PED YES CDM-3, PED-2 RECOMMENDED DX-320 with IC20 or IC25 RECOMMENDED DX-320 with IC25A NO DX-500 RECOMMENDED DX-600 with CD25A or ED50A NO DX-600 with CD25 or ED50 RECOMMENDED DX-800 RECOMMENDED ICS-90 N/A ICS-1000 NO ICS-1500 NO ICS-2000 NO ICS-2500 NO ICS-3000 NO

14 SRS 300 Product Manual Page 13 of 50 The SRS 300 is installed in the column chamber of the chromatography module immediately after the analytical column and before the conductivity detector cell. All components required for installation of the SRS 300 are included with the system. Gas Separator Waste Tube (P/N ) Backpressure coil(s) 4-mm (P/N ) 2-mm (P/N ) Microbore Tubing (2-mm only) (P/N ) Mounting clip (P/N ) Options: MMS/SRS Installation Kit (P/N ) (Pressurized Water Delivery System used with AutoSuppression External Water Mode, Chemical Suppression Mode, or MPIC Suppression Mode) Peristallic Pump Kit (P/N: ). (Water delivery system used with AutoSuppression External Water Mode, Chemical Suppression Mode or MPIC Mode. CAUTION The SRS 300 must be operated with the Gas Separator Waste Tube (P/N ) NOTE The use of 1/4-28 or ferrule/bolt style liquid lines may be required for installation and use of SRS 300. See Dionex Liquid Line Fittings for complete details Self-Regenerating Suppressor Control The SRS control is provided by discreet (50,100,300 and 500mA) and non discreet (0 to 500 ma in 1mA increment) power supplies. Discreet SRS Control is integrated into the CDM-3 and PED-2 of the DX-300, the DX-100 (Model 1-03), DX-120, DX-320 (IC20 and IC25 models), DX-500 (CD20 and ED40 detectors), and DX-600 (CD25 and ED50 detectors). For applications that require intermediate current values the use of a non-discreet power supply, such as the SC20, RFC-10 or RFC-30 is highly recommended. Non-discreet SRS Control is integrated into modern instruments including the DX-320 (IC25A model), DX-600/ICS-2500 (CD25A and ED50A detectors) and ICS series (excluding ICS-90 and ICS-900). CAUTION Always turn the pump and the SRS Control on and off at the same time. Eluent flow through the SRS 300 is required for proper operation. However, without current, the membranes and screens in the SRS 300 will become expended by the flowing eluent resulting in small analyte peak areas. If this should occur, perform the procedure in Section Reagent-Free Controller (RFC) The Reagent-Free Controller (RFC) is an external power supply available in two versions. The RFC-10 controls the SRS 300 Self-Regenerating Suppressor or an AES Atlas Electrolytic Suppressor. Current is delivered at 1 ma resolution. The RFC-30 controls an SRS 300 Self-Regenerating Suppressor or AES, as well as an EluGen Eluent Generator Cartridge (EGC) and a CR-TC Continuously Regenerated Trap Column. Current is delivered at 1 ma resolution. The RFC controls these devices by supplying current to the suppressor and for the RFC-30, current to the eluent generator and voltage (to the CR-TC). Please see the RFC Operator s Manual for suppressor operating and installation instructions with the following Dionex products: DX-320/320J DX-500, DX-600, or ICS-2500 DX-120

15 SRS 300 Product Manual Page 14 of Back Pressure Coils for the SRS 300 All detector cells require enough back pressure to prevent eluent in the cell from out-gassing due to abrupt volume changes between the small inner diameter of the connecting tube and the relatively larger volume of the cell. Out-gassing creates bubbles in the cell and disrupts detector responsiveness. Back pressure coils help to prevent gases, generated during AutoSuppression, from out-gassing and formation of bubbles in the detector cell. For example, carbonate eluent is suppressed to carbonic acid which is CO 2 gas in equilibrium with DI water and CO 2 gas can come out of solution if adequate pressure is not applied. The above out-gassing can trap bubbles in the cell causing high noise. Therefore Dionex recommends addition of psi of backpressure. Back pressure coil components are shipped with your system. For 4 -mm systems, locate assembly P/N For 2 -mm systems, the backpressure coils are also available in the microbore tubing kit, P/N For 2- mm systems, locate assembly P/N Alternatively, lengths and diameters of tubing necessary for proper back pressure are given in Table 3, Coils for SRS 300 Back Pressure Requirements. Adjust the tubing length to achieve a backpressure of approximately 40 psi. CAUTION If back pressure coils become damaged or plugged, they may cause irreversible damage to the suppressor Assembly A. Slip PEEK liquid line bolts and ferrules onto the ends of the tubing. Refer to Table 3, Coils for SRS 300 Back Pressure Requirements, and determine the correct number of coils required for your application based on the eluent flow rate. B. After assembly of the coils, see Figure 7, The AutoSuppression Recycle Mode Plumbing Diagram, for the proper placement of the completed coils and couplers between the SRS 300 and the Gas Separator Waste Tube. Table 3 Coils for SRS 300 Back Pressure Requirements SRS 300 Type P/N Flow Rate I.D. of Tubing Length of Each Coil Number of Coils 4-mm ml/min 0.010" (Black) 2.5 ft. 2 4-mm ml/min 0.010" (Black) 2.5 ft. 1 2-mm ml/min 0.005" (Red) 1.0 ft. 2 2-mm ml/min 0.005" (Red) 1.0 ft. 1 CAUTION The correct amount of back pressure for optimum operation is 40 psi. Back pressure over 150 psi after the SRS 300 can cause irreversible damage.

16 SRS 300 Product Manual Page 15 of Gas Separator Waste Tube for the SRS 300 The Gas Separator Waste Tube (P/N ) is an integral part of the SRS 300 system. It separates any hydrogen gas generated in the ASRS 300 during the electrolytic generation of hydronium ions (H3O+) or hydroxide ions (OH-) for the CSRS 300. The Gas Separator Waste Tube is used to avoid concentrating the gas in the waste container. The Gas Separator Waste Tube is shipped in one of the ShipKits of your system. CAUTION Do not cap the waste reservoir. SAFETY Minimal hydrogen gas generated by the SRS 300 is not dangerous unless the gas is trapped in a closed container and allowed to concentrate. The Gas Separator Waste Tube must be open to the atmosphere, and not in a confined space, to operate properly Assembly Assemble and install the Gas Separator Waste Tube and waste line following the steps below. See Figure 5, The AutoSuppression Recycle Mode Plumbing Diagram, or Figure 7, Configuration of the Pressurized Water Reservoir and the Gas Separator Waste Tube with the Self-Regenerating Suppressor. A. Use one or two couplers (P/N ) to connect two or three lengths of 1/2" i.d. black polyethylene tubing (P/N ) depending on the waste container depth. Extend the top of the Waste Separator Tube above the top of the Waste container. Place the Gas Separator Waste Tube with the 1/8" o.d. tubing attached into the waste container. Ensure the bottom of the Gas Separator Waste Tube is resting on the floor of the waste container, the top of the device (where the white 1/8" o.d. tubing meets the black 1/2" o.d. tubing) is above the top of the container, and that both the Gas Separator Waste Tube and the waste container are open to the atmosphere Self-Regenerating Suppressor Current Selection Lower current is better for the performance of both the SRS 300 and Atlas suppressors. Excess current through the suppressor devices causes excess heat generation and over time will cause the ion exchange materials to degrade, thus shortening suppressor lifetime. Excess current can also cause poor recoveries of certain analytes, particularly magnesium, manganese and phosphate. The optimum current setting produces just enough hydronium or hydroxide ions to displace the eluent counter ions and neutralize the eluent and is the recommended setting. No more than 10% above the optimum current setting is recommended.

17 SRS 300 Product Manual Page 16 of Calculating the Optimum Current Setting The optimum current setting depends on the eluent concentration and flow rate. A concentrated eluent at a high flow rate requires a higher current setting than a diluted eluent at a low flow rate. These calculations are specific for the type of suppressor and vary for ASRS 300 and CSRS 300. Current (ma) = [flow rate (ml/min)] x [eluent concentration (mn)] x [a suppressor specific factor] The factors are listed in the table below. The unit for eluent concentration is mn (not mm). Table 4 Optimum Suppressor Settings Suppressor Type Suppressor Specific Factor ASRS CSRS Atlas (Anion and Cation) 3.34 NOTE Always round the calculated optimum current up to the nearest whole integer.

18 SRS 300 Product Manual Page 17 of 50 An RFC-10 or RFC-30 Controller, CD25A, ED50A, IC25A, ICS-1000, ICS-1500, ICS-2000, or ICS-3000 detector can be used to set the current at the calculated value with a minimum current resolution of 1 ma. NOTE The lower flow rates require a lower current. A 2 mm SRS 300 should NEVER be operated at a current above 100 ma. A. Maximum Suppression Capacity The Maximum Suppression Capacity (MSC) depends on the eluent concentration and flow rate. The MSC can be calculated using the following equation. MSC (mn * ml/min) = flow rate (ml/min) * sum of eluent concentration (mn) Table 5 Maximum Suppression Capacity for SRS 300 Suppressor Flow Rate (ml/min) Maximum Suppression Capacity ASRS mm µ equivalents ASRS mm < 50 µ equivalents ASRS mm < 30 µ equivalents CSRS mm < 100 µ equivalents CSRS mm < 35 µ equivalents CSRS mm µ equivalents B. Sum of Eluent Concentration Calculation The sum of the eluent concentration can be calculated from the equations below. ASRS 300 (4-mm) Sum of eluent concentration (mn) = {2* Carbonate (mm) + Bicarbonate (mm) + hydroxide (mm) + 2 * Tetraborate (mm) + custom eluent cation (mn)} where Tetraborate is <= 50 mm ASRS 300 (2-mm) Sum of eluent concentration (mn) = {2 * Carbonate (mm) + Bicarbonate (mm) + hydroxide (mm) + 2 * Tetraborate (mm) + custom eluent cation (mn)} where Tetraborate is <= 75 mm Custom eluent cation (mn) can be calculated from the normality of the eluent concentration. NOTE Normality is Equivalents/L of solution. For example, 20.0 mm sodium acetate (CH3COONa) has 20.0 mn sodium as the cation and 20.0 mm sodium sulfate (Na2SO4) has 40.0 mn sodium as the cation. When using the CSRS 300 (4-mm) and CSRS 300 (2-mm), the sum of the eluent concentration can be calculated using the equations below. CSRS 300 Sum of eluent concentration (mn) ={2 * Sulfuric Acid (mm) + MSA (mm) + custom eluent anion (mn)} Custom eluent anion (mn) can be calculated from the normality of the eluent concentration. NOTE Normality is Equivalents/L of solution. For example, 20.0 mm sodium acetate (CH3COONa) has 20.0 mn acetate as the anion and 20.0 mm sodium sulfate (Na2SO4) has 40.0 mn sulfate as the anion.

19 SRS 300 Product Manual Page 18 of OPERATION This section provides instructions for the start-up and operation of the SRS 300 including the selection process and suppression modes of operation Chemical Purity Requirements Precise and accurate results require eluents free of ionic impurities. Chemicals and deionized water used to prepare eluents must be pure as described below. Low trace impurities and low particulate levels in eluents and regenerants also help protect the SRS 300 and system components from contamination. SRS 300 performance is not guaranteed when the quality of the chemicals and water used to prepare eluents has been compromised Inorganic Chemicals Reagent Grade inorganic chemicals should always be used to prepare ionic eluents. Preferably, a lot analysis on each label will certify each chemical as meeting or surpassing the latest American Chemical Society standard for purity, a universally accepted standard for reagents Solvents Since solvents used with the SRS 300 are added to ionic eluents to modify the ion exchange process or improve sample solubility, the solvents used must be free of ionic impurities. However, since most solvent manufacturers do not test for ionic impurities, the highest grade of solvents available should be used. Currently, several manufacturers are making ultra-high purity solvents that are compatible for HPLC and spectrophotometric applications. These ultra-high purity solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent. Dionex has obtained consistent results using High Purity Solvents manufactured by Burdick and Jackson and Optima Solvents by Fisher Scientific Deionized Water The deionized water used to prepare eluents should be degassed Type I Reagent Grade Water with a specific resistance of 18.2 megohm-cm. The water used for the AutoSuppression External Water Mode should have a specific resistance of 18.2 megohm-cm or greater. The deionized water should be free of ionized impurities, organics, microorganisms and particulate matter larger than 0.2 µm. It is good practice to filter eluents through a 0.2 µm filter whenever possible. Bottled HPLC-Grade Water should not be used since most bottled water contains an unacceptable level of ionic impurities. Finally, thoroughly degas all deionized water prior to preparing any eluents or regenerants Start-up The SRS 300 is installed in the column chamber of the chromatography module right after the analytical column and before the conductivity detector cell. On the ICS-3000, the suppressor mounts on the conductivity detector module in the DC. On the ICS-2000, the ICS-1500, and the ICS-1000, the suppressor mounts on the component panel behind the ICS front door. Refer to the ICS Operator's Manual for further details. On the DX-500, DX-120, and DX-100 instruments, the SRS 300 mounts on tabs on the component panel. Orient the SRS 300 with the ELUENT IN port and the cable at the top; align the slots on the back of the SRS 300 with the tabs on the panel. Press in, and then down, to lock the SRS 300 in place. Lift up and pull out to remove the SRS 300. Ensure the SRS 300 is plumbed properly according to the selected mode of operation. Refer to Section 2, Installation, for complete installation instructions. WARNING Keep the regenerant chambers full with the appropriate regenerant solution or water. The membranes and screens in the SRS 300 must be completely hydrated to maintain liquid seals and chromatographic performance. CAUTION The correct amount of back pressure for optimum operation is 40 psi. Connect the back pressure coil(s) appropriate for your column i.d. and flow rate. Back pressures over 150 psi after the SRS 300 can cause irreversible damage.

20 P / N SRS 300 Product Manual Page 19 of 50 CAUTION Do not cap the waste reservoir. SAFETY Hydrogen gas generated by the SRS 300 is not dangerous unless the gas is trapped in a closed container and allowed to concentrate. The Gas Separator Waste Tube must be open to the atmosphere, and not in a confined space, to operate properly Hydration 1. Hydrating the suppressor ensures that the ion exchange membranes are in a swollen form for proper operation. A 20 minute static step is recommended during first time installation to ensure complete hydration. 2. Using a disposable plastic syringe and the Luer adapter (P/N ), push approximately 3 ml (SRS 4-mm) or 0.75 ml (SRS 2-mm) of degassed DI water through the ELUENT OUT port. Using a disposable syringe and the 1/4-28 Luer adapter (P/N ), push 5 ml (SRS 4-mm) or 2 ml (SRS 2-mm) of degassed DI water through the REGEN IN port, according to Figure 6. NOTE Step 1 can be accomplished by installing the suppressor in the system in the recycle mode, bypassing the guard and analytical columns, and pumping 5 ml (SRS 4-mm) or 2 ml (SRS 2-mm) of deionized water through the suppressor. P/N Description cc plastic syringe /4-28 Luer adapter Luer adapter Union Bolt Double Cone Ferrule 1C C 1.0 c c s yringe Bolt and Ferrule L u e r a d apter Union ELUENT IN REGENOUT DIONEX ANION SELF-REGENERATING SUPPRESSORASRSULTRA 4-mm ELUENTOUT REGEN IN D I H 2 O D IH 2 O Figure 6 Hydrating the Suppressor 3. Allow the suppressor to sit for approximately 20 minutes to fully hydrate the suppressor screens and membranes. WARNING Do not install a luer adapter directly into a SRS 300 port. Connect a luer adapter to a union and use two bolt and ferrules with a few centimeters of tubing to connect to the SRS ports.

21 SRS 300 Product Manual Page 20 of Back Pressure Coil Pressure Test 1. Disconnect the eluent line from the injection valve to the column at the column inlet. Injection Valve 2. Connect the eluent line from the injection valve directly to the detector cell inlet with the recommended number of back pressure coils attached for your application (see the table below). Turn the pump on at your application flow rate. After 2 to 3 minutes of equilibration record pressure P Disconnect the back pressure coils and with the pump on measure the system pressure P 2. Coil #1 Cell Coil #2 4-mm Chromatography 2-mm Chromatography Waste 1.0 ml/min. = 2 black backpressure coils 0.25 ml/min. = 2 red backpressure coils (P/N ) (P/N ) 2.0 ml/min. = 1 black backpressure coil 0.50 ml/min. = 1 red backpressure coil (P/N ) (P/N ) 4. The correct operating pressure range for the backpressure coil being tested is Injection Valve SRS 300 P 1 - P 2 = psi If the pressure is greater than 40 psi, then trim the back pressure coil and repeat step 2 and 3 to achieve psi in step 4. Cell If it is less than 30 psi, then add more tubing to achieve psi Quick Back Pressure Check Waste This section describes how to measure the backpressure to the suppressor. Install the system for the application of choice. 1 Measure the system pressure P1 with the suppressor powered 2. Unplug the line from the Eluent Out port on the suppressor and measure system pressure P 2 CAUTION Do not leave the port open for more than 2 minutes. 3. P 1 -P 2 < 100 psi. 4. Adjust the backpressure coils if needed to achieve the < 100 psi value. Refer to to measure the back pressure contribution from the back pressure coil.

22 SRS 300 Product Manual Page 21 of Plumbing for the AutoSuppression Recycle Mode Operation Figure 7 The AutoSuppression Recycle Mode Plumbing Diagram The AutoSuppression Recycle Mode is the easiest method of operation. As the eluent passes through the suppressor, it is neutralized to produce its weakly ionized form. After passing through the conductivity cell, this effluent can be redirected to the regenerant inlet on the suppressor, thus supplying it with a source of water containing a small amount of diluted analyte (see Figure 7). The main advantage of this mode is its simplicity and ease of use. It is not necessary to have an external supply of water available for the suppressor. CAUTION Only use the AutoSuppression Recycle Mode for eluents without organic solvents or metallic contaminants such as iron in ground water Eluent Flow Path Connections in the AutoSuppression Recycle Mode Depending on the specific components (analytical column, conductivity cell, back pressure coils) in the system, 1/4-28 or ferrule/bolt liquid lines may be required. All necessary tubing and fittings are supplied in the detector or RFC-10 or RFC- 30 Ship Kits. To purchase or assemble 1/4-28 or ferrule/bolt liquid lines, refer to, Dionex Liquid Line Fittings. Always use 0.005" i.d. PEEK tubing with ferrule/bolt fittings on 2 mm systems. Use 0.010" i.d. PEEK tubing with ferrule/bolt fittings on 4 mm systems when possible. Avoid adding dead volume to the system by keeping all eluent lines as short as possible. A. Install the SRS 300 inside the ICS Module. B. Connect the outlet of the analytical column to the ELUENT IN of the SRS 300 (Figure 7). C. Connect the ELUENT OUT port of the SRS 300 to the inlet of the conductivity cell (Figure 7).

23 SRS 300 Product Manual Page 22 of Regenerant Flow Path Connections in the AutoSuppression Recycle Mode Connect the back pressure coil(s) between the CELL OUTLET port and the REGEN IN port (see Figure 7 and Section 2). The back pressure coils are provided in the Gas Separator Waste Tube Components Assembly (P/N ) for 4-mm systems. The backpressure coils for 2-mm systems are provided in the microbore tubing kit (P/N ). CAUTION The SRS 300 must be operated with the Gas Separator Waste Tube (P/N ) Installation in Thermal Chamber A. Installation instructions for single temperature zone ICS-3000 DC. 1. For all applications up to 35 C the suppressor is installed inside the heated DC enclosure. Install the suppressor using the suppressor holder on the CD. 2. For applications above 35 C up to 40 C, it is recommended the SRS 300 is installed outside the DC. B. Installation instructions for dual temperature zone ICS-3000 DC. 1. Install the suppressor using the suppressor holder on the CD in the upper compartment. Ensure the upper compartment temperature is set to a value no greater than 35 C and temperature control is turned on. It is recommended that the upper compartment is kept cooler than the lower compartment. The lower compartment (column oven) can be set to temperatures up to 70 C. C. Installation instructions for ICS 1000/1500/2000, AS50 thermal chamber TC and CC: 1. Install the suppressor using the suppressor holder. The suppressor is installed outside the heated column enclosure. It can support all high temperature applications up to 60 C. D. Installation instructions for LC30 and LC25 ovens: 1. For all ANION applications up to 35 C, install the suppressor in the oven using the SRS holder. 2. For operation above 35 C and up to 60 C, it is recommended that the ASRS 300 suppressor be installed outside the oven. This would ensure optimal performance of the suppressor in terms of noise and background. 3. For all CATION applications up to 40 C, install the suppressor in the oven using the SRS holder. 4. For operation above 40 C and up to 60 C, it is recommended that the CSRS 300 suppressor be installed outside the oven. This would ensure optimal performance of the suppressor in terms of background and noise. NOTE Operating the suppressor by installing the suppressor inside a column/thermal compartment or oven over 35 C will physically damage the suppressor. Set the required current based on your specific application requirements for column flow rate and temperature in addition to eluent concentration. If using Chromeleon software, the Wizards can greatly assist you in determining the correct requirements. Refer to Section 2 for suppressor current calculations and Appendix A for examples Installation in ICS 3000 In the single-zone (shared) configuration of the Detector Compartment (DC) module of the ICS 3000 system, the upper and lower compartments are at the same temperature. The suppressor should be installed in the upper compartment. In the dual-zone configuration of the DC module the upper and lower compartments have independent thermal control. The suppressor should be installed in the upper compartment. The allowed temperature setting for the upper compartment is 35 C

24 SRS 300 Product Manual Page 23 of Plumbing for the AutoSuppression External Water Mode Operation Figure 8 The AutoSuppression External Water Mode Plumbing Diagram Any analysis that can be performed using the AutoSuppression Recycle Mode can be done using the AutoSuppression External Water Mode. A constant source of deionized water having a specific resistance of 18.2 megohm, or greater, is supplied to the regenerant chambers to generate hydronium or hydroxide ions for neutralization. CAUTION AutoSuppression External Water Mode is used when organic solvents are present in the eluent. When the SRS 300 is operating in the AutoSuppression External Water Mode, the background noise may be lower than in the AutoSuppression Recycle Mode because the external water flow rate is not limited to the eluent flow rate. The independent source of external water allows for higher water flow rates and better sweep out of bubbles from the Regen chamber resulting in lower background noise Eluent Flow Path Connections for the AutoSuppression External Water Mode Depending on the specific components in the system (such as analytical column, conductivity cell, back pressure coils), 1/4-28 or ferrule/bolt liquid lines may be required. All necessary tubing and fittings are supplied in the detector or RFC-10 or RFC-30 Ship Kits. To purchase or assemble 1/4-28 or ferrule/bolt liquid lines, refer to, Dionex Liquid Line Fittings. Always use 0.005" i.d. PEEK tubing with ferrule/bolt fittings on 2 mm systems. When possible, use 0.010" i.d. PEEK tubing with ferrule/bolt fittings on 4 mm systems. Avoid adding dead volume to the system by keeping all eluent lines as short as possible. A. Install the SRS 300 in the first slot inside the Chromatography Module. B. Connect the outlet of the analytical column to the ELUENT IN of the SRS 300 (Figure 8).

25 SRS 300 Product Manual Page 24 of 50 C. Connect the ELUENT OUT port of the SRS 300 to the inlet of the conductivity cell (see Figure 8). D. Install a waste line from the conductivity cell that generates 40 psi back pressure at the flow rate required by the application. Use the appropriate i.d. tubing depending on your application requirements. Refer to Section 2 and see Figure 7 for the correct back pressure tubing requirements. E. Install and adjust the flow rate of water from the pressurized water delivery system to the regenerant chambers of the SRS 300 (see Section 3). CAUTION The correct amount of back pressure for optimum operation is 40 psi. Back pressures over 150 psi can cause irreversible damage Regenerant Flow Path Connections in the AutoSuppression External Water Mode The SRS 300 Pressurized Bottle Installation Kit (P/N ) contains all of the components needed to install and operate the SRS 300 with a pressurized water reservoir. The kit contains the SRS Installation Parts Kit (P/N ), a 25 psi regulator (P/N ) and a 4 liter water reservoir (P/N ). A. Make the following air line connections: 1. Locate the pieces of tinted 1/8" o.d. plastic tubing (P/N ) supplied in the Installation Parts Kit. 2. Push the end of one piece of 1/8" o.d. tubing over the barbed fitting of the regulator. Connect the other end of the tubing to the source of air pressure. 3. Push one end of the second piece of 1/8" o.d. tubing over the other barbed fitting of the regulator. Push the other end of this tubing over the barbed fitting (P/N ) in the pressure inlet of the plastic reservoir (see Figure 13). B. Make the following water line connection. 1. Use a coupler (P/N ) to connect one end of the 30" tubing assembly (P/N ) that comes in the Installation Kit to the water reservoir. Connect the other end of this tubing to the REGEN IN port of the Self- Regenerating Suppressor. 2. Using a coupler (P/N ) and a 1/8" o.d. piece of tubing (P/N ) from the Installation Kit, connect one end of this line to the REGEN OUT port of the SRS 300 and then connect the other end of the line to the Gas Separator Waste Tube. C. Fill the water source reservoir. Make sure that the O-ring is inside the cap of the reservoir before screwing the cap onto the reservoir. Screw the cap onto the reservoir tightly and place the reservoir near the Chromatography Module. D. With no current applied, adjust the external water flow rate to approximately 3 5 ml/min for the SRS 300 (4-mm) and 1 3 ml/min for the SRS 300 (2-mm) by using a graduated cylinder and measuring the flow from the REGEN OUT waste line. The pressure applied to the reservoir can vary from 0 25 psi (the lower and upper pressure limits of the water reservoir) but the typical operating pressure is between psi. Please note that this value is highly system dependent. After turning on the current, the external water flow rate will be less because the electrolysis of water will generate a small amount of hydrogen and oxygen gases that will be seen as bubbles from the REGEN OUT waste line. In summary, the final external water flow rate is dependent on two factors: the pressure applied to the water reservoir and the current setting. It is best to measure it with the current off since the formation of bubbles will decrease the accuracy of the overall measurement. SAFETY A safety relief valve on the reservoir regulator prevents pressure greater than 25 psi from being applied to the water reservoir.